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Technische Universität München> Technische Universität MünchenHelmholtz-Zentrum Hereon> Helmholtz-Zentrum Hereon
Forschungszentrum Jülich> Forschungszentrum Jülich

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85748 Garching

KWS-X: The SAXS/WAXS Laboratory Beamline

SAX Labor Overview SAX Labor Overview SAXS-WAXS laboratory beamline front view. © Baohu Wu /JCNS-MLZ

SAXS-WAXS laboratory beamline front view. © Baohu Wu /JCNS-MLZ

The customized small- and wide-angle X-ray scattering (SAXS/WAXS) instrument from XENOCS has been installed in the 45 m2 SAXS lab since the end of 2021. As one of the most powerful in-house SAXS instruments in the world, it offers highly complementary experimental capabilities to our SANS and other neutron instruments. The lab is also equipped with sample preparation tables, sample environment platforms, and various supporting facilities.

As a young member of our small-angle scattering instruments using X-ray as the beam, KWS-X is equipped with a high flux metal-jet source and a moveable Eiger 2R 4M SAXS detector. With an additional 4-axis motorized WAXS detector and Bonse-Hart USAXS, the scattering vector q can cover a wide area from 0.0002 to 7 Å-1. Compared to other instruments, it also comprises a large sample environment station that can be used with ambient pressure conditions. Many sample environmental accessories make it possible to perform experiments at temperatures from -150oC to 1000oC, under shear, tensile, etc.

The KWS-X SAXS-WAXS-USAXS beamline has been commissioned and officially opened to users in April 2023. In addition to being a complementary method to SANS, it will also provide users with testing services before experiments on neutron scattering instruments (SANS instruments KWS-1, KWS-2, KWS-3 and other neutron scattering instruments). This will greatly help users optimize neutron scattering samples and greatly improve the efficiency of SANS experiments. In addition, KWS-X can also use X-ray to debug large neutron sample environments.

Technical Data

X-ray source
• Excillum’s MetalJet D2+
• Ga anode 250W 70kV 3,57 mA 20×80 μm
• Flux
~2.45×109 ph/s Full beam model;
~ 6.16×108 ph/s High Flux (HF) model;
~ 8.09×107 ph/s High Resolution (HR);
~ 1.77×106 ph/s Ultra High Resolution (UHR)

Optics and Collimation
FOX 3D Galium multilayer optics
• Slightly focusing optics
• Four motorized independent blades per set of slits (S1, S2 and S3)
• S1 + S3: Collimation length> 1.9 m (Sample chamber or BioCUBE)
• S1 + S2: Collimation length> 1.3 m (XL position)

SAXS Detector: Dectris Eiger2R 4M
• Pixel Size: 75× 5 µm²
• 4,5 Million pixels
• Sensitive Area: 155×163 [mm²]
• Modules (W x H): 2×4
• Countrate capability: 10⁷ ph/s/pixel
• Q-Xoom: in-vacuum moving detector
• Sample to detector distance > 1.8 m

WAXS Detector: Dectris Eiger2R 500K
• Pixel Size: 75 × 75 µm²
• 4-axis motorized WAXS for simultaneous 2D WAXS measurements

BONSE-HART USAXS
• Monochromator: 2-bounce Bartels Si(111)
• Analyzer: 4-bounce Si(111) channel cut crystals

Features

Wide Q range
SAXS: 0.0015 Å-1 < q < 5 Å-1
USAXS: qmin < 0.0002 Å-1
WAXS: qmax > 7 Å-1

High flux and lower background level
• Possible for time-resolved experiments in second level
• Allow low concentration samples

Three main measurement positions with maximum flexibility
• Sample chamber, BioCUBE and XL position
• Measurements in vacuum or in air
• Modular conversion of various settings Sample chamber/BIOCUBE/XL
• Plenty of space for large sample environment.

In-line sample visualization
• 2xCCTV in-line camera + 3 overview camera + 1 endoscope
• Machine vision technology

Sample Environment,Add-ons and Lab Equipments

Standard sample holders
• 27 positions 1.5 mm capillary holder
• 27 positions 2.0 mm capillary holder
• 25 positions Solids sample holder
• 61 positions Solids sample holder
• 15 positions powder/gel sample holder
• 8 positions powder/gel capsule sample holder (0.5 mm and 1 mm spacer)

Temperature controlled sample holders
• Multi-purpose Temperature Stage (-30 – +150°C)
• Multi-refillable capillary holder with temperature control (-10°C to +80°C)
• Linkam temperature stage MFS350 (capillaries & flat cells, -150 to +350°C)
• Linkam extended high temperature sample stage (RT to 1000°C)

Flow cells
• Low Noise flow cell (SiN windows)
• Glass capllary flow cell (ID from 1 mm to 4 mm)
• Polyconbonate capllary flow cells (ID 2 mm)
• BioCUBE flow cell Assembly & cleaning pump system & HPLC connection

Shear and Rheo-SAXS
• Linkam Shear Cell System (-50 to 350°C)
• Anton paar Rheometer- Polyconbonate double cylinder shearing system

Tensile
• Linkam Modular Force Stage

Surface and interface
• Standard and advanced GISAXS/GIWAXS module

Humidity control
• Xenocs Humidity control and generator (1 RH% to 95 RH%)

Magnetic field
• Permanent magnet (Halbach) arrays > 0.6 T

UV/Vis
• In-line UV/Vis spectrometer for BioCUBE

pH control
• Metrohm Trtrtion system and reaction cell, pH-counter ion control system

BIOSAXS system
• BioXolver and Cart for auto sample loading robot plus capillary flow cells

SEC-SAXS
• In line SEC-SAXS set up by conbination of a HPLC system and the BioCUBE flow cell.

Add-ons
• Linkam T96 controller and Lquid Nitrogen pump
• XL Large sample environment station, capacity > 100 kg
• Additional rotation capability for the XL- XZ table
• mT Jumping and stopped flow/ UV-Vis/ Fluorescence

More sample environments from our neutron instrument can be shared with our neutron sample environments. Users can also bring their own sample environment.

Lab Equipments

MIG-O-MAT Lötstar 141: Micro Soldering and Welding Unit for capillary sealing
• Julabo F25-HE refrigerated circulator
IKA VORTEX 3 and accessories
• Reglo ICC Digital Peristaltic Pump
• Micro Hämatokrit (capillary) centrifuge
• Laboratory refrigerator
• Variomag Mini Stirrer
• PC 3001 VARIOproVARIO chemistry pumping unit
• Metrohm pH Meter 913
IKA magnetic stirrer with heating
• Emag 12 HC Ultraschallreiniger 100 W 1.2 l
PCE-BT 200 precision scale weighing 0.001g- 210 g (max.)

Applications

Life and medical science
• Structure and interactions of protein, nucleic acid
• In-situ monitoring of protein conformational changes, protein aggregation
• Characterizing monoclonal antibody-protein antigen interactions
• Hierarchical structures of biomaterials, e.g. collagen, chitosan
• Drug delivery systems based on nanoparticles, vesicles or liposomes

Polymer and soft matter
• Structure of polymers, colloids, hydrogels, surfactants and micellers
• In-situ crystallisation of semi-crystalline polymer
• Determine the phase of self-assembled block-copolymers or liquid crystalline polymers
• Test the tensile properties of polymer or follow the degree of crystallinity
• Microemulsions, complex fluids …
• Colloids, nanocomposites, polymer gels …

Material science
• Structure of fibre, membranes, thin films and nanocomsposites …
• Aerogels, silica foams, coating
• Micro and mesoporous materials, cements, metal and alloys
• Crystal formation during perovskite deposition and other energy materials

Food science
• Monitor the size, shape and stability of fat globules in dairy upon aging, drying and digestion
• Crystalline fraction and lamellar structure in starchy
• Structure and size of polysaccharides and proteins in hydrated systems
• Oleo-gelator network

How to apply beamtime

The KWS-X SAXS-WAXS beamline invites applications from universities, research institutes, and industries worldwide. There are currently three ways to apply:

Via MLZ Neutron Scattering Proposal: When submitting a neutron scattering beamtime proposal through the MLZ system, you can also apply to use the KWS-X SAXS-WAXS beamline as an additional method in the Ghost system. If your neutron proposal is accepted and there are no technical issues, your KWS-X application will also be approved.

Direct Application Through Collaboration: You may apply directly for KWS-X beam time in collaboration. It is recommended to consult with the instrument manager before applying. Once approved, the experiment can be conducted remotely by mailing samples or performed on-site.

For Industrial Users: Industrial users are welcome to contact us directly to apply for access to the instruments.

Contact

Dr. Baohu Wu (Head)
Email: ba.wu@fz-juelich.de
Phone: +49 (0)89 158860-687

SAXS Labor (KWS-X, UYL 122)
Phone: +49 (0)89 158860-122

KWS-X: The new SAXS/WAXS Laboratory Beamline

SAXS-WAXS laboratory beamline overview.

The new SAXS-WAXS laboratory beamline. © MLZ

Read more

Gallery

SAXS-WAXS laboratory beamline from Metal-jet source view.

© Baohu Wu/FRM II
04_SAXS-WAXS
04_SAXS-WAXS

SAXS detector in the detector chamber.

© MLZ
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10_SAXS-WAXS

Sample measuring in open-air position XL.

© MLZ
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09_SAXS-WAXS

USAXS Analyzer move out in sample chamber.

© MLZ
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08_SAXS-WAXS

SAXS-WAXS beamline in the laboratory.

© MLZ
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06_SAXS-WAXS

Peltier stage in sample chamber.

© MLZ
07_SAXS-WAXS
07_SAXS-WAXS

BIOSAXS Robot autosampler.

© MLZ
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03_SAXS-WAXS

SAXS-WAXS laboratory beamline from top view.

© MLZ
05_SAXS-WAXS
05_SAXS-WAXS

SAXS-WAXS laboratory beamline overview.

© MLZ
01_SAXS-WAXS
01_SAXS-WAXS

SAXS-WAXS laboratory beamline overview.

© MLZ
02_SAXS-WAXS
02_SAXS-WAXS

SAXS-WAXS laboratory beamline from right side view.

© MLZ
KWS-X-LAB-instrument-view
KWS-X-LAB-instrument-view
KWS-X-SEC-SAXS
KWS-X-SEC-SAXS
KWS-X-XL-set-up
KWS-X-XL-set-up
KWS-X-XL-TR-REAC-CELL
KWS-X-XL-TR-REAC-CELL
KWS-X-High-TEMP
KWS-X-High-TEMP

MLZ is a cooperation between:

Technische Universität München> Technische Universität MünchenHelmholtz-Zentrum Hereon> Helmholtz-Zentrum Hereon
Forschungszentrum Jülich> Forschungszentrum Jülich

MLZ is a member of:

LENS> LENSERF-AISBL> ERF-AISBL

MLZ on social media: